A high molecular weight poly(2,2'-dithiodianiline) (PDTDA) was chemically synthesized by simple solution polymerization method. The weight average molecular weight ((M) over bar (w)) was observed to be 424,690 by GPC analysis. The chemical structure of the undoped PDTDA was characterized by UV/VIS spectroscopy. It was confirmed that the S-S bonds within repeating units could be conserved well after chemical polymerization by FTIR spectroscopic analysis.